This
work evaluates the use of nanosecond laser ablation–multicollector
inductively coupled plasma-mass spectrometry (ns-LA–MC-ICP-MS)
for Fe isotopic analysis of glassy cosmic spherules. Several protocols
for data acquisition from the transient signals were compared, with
the integration method, i.e., isotope ratios obtained by dividing
the corresponding signal intensities integrated over the selected
signal segment, providing the best precision. The bias caused by instrumental
mass discrimination was corrected for by a combination of internal
correction using Ni as an internal standard (coming from a conebulized
standard solution) and external correction using a matrix-matched
standard. Laser spot size and repetition rate were adapted to match
the signal intensities for sample and standard within ±10%. For
in situ isotopic analysis, the precision of the δ56Fe values ranged between 0.02 and 0.11‰ (1 SD, based on 4
measurement sessions, each based on ablation along 5 lines for 30
s each) and 0.03–0.17‰ (SD, based on 3 measurement sessions)
for glass reference materials and micrometeorites, respectively. Despite
this excellent reproducibility, the variation of the isotope ratios
along a single ablation line indicated isotopic inhomogeneity exceeding
1‰ in some micrometeorites. Isotopic analysis via pneumatic
nebulization MC-ICP-MS, after sample digestion and chromatographic
Fe isolation, was performed to validate the results obtained by in
situ isotopic analysis, and good agreement was achieved between the
δ-values
obtained via both approaches and with those reported in literature
for MPI-DING and USGS glass reference materials. Also for the glassy
cosmic spherules, overall, there was a good match between the ns-LA–MC-ICP-MS
and solution MC-ICP-MS results.